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A system and preparation method for preparing methyl phosphite by using methylaluminum chloride

A technology of methyl phosphite and methyl aluminum chloride, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of low product yield, increased side reactions, etc. The problem of high cost of product purification, to achieve the effect of improving the reaction rate, improving the production efficiency, and improving the simplicity

Active Publication Date: 2022-02-22
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0010] Aiming at the problems that the existing technology cannot continuously prepare methyl phosphite, the product yield is low, the side reactions increase, and the product purification cost is high, the present invention provides a system and a method for preparing methyl phosphite by using methylaluminum chloride. Preparation

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  • A system and preparation method for preparing methyl phosphite by using methylaluminum chloride
  • A system and preparation method for preparing methyl phosphite by using methylaluminum chloride
  • A system and preparation method for preparing methyl phosphite by using methylaluminum chloride

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preparation example Construction

[0141] The preparation method comprises the following steps:

[0142] (a) raw material aluminum, catalyzer and gasified methyl chloride carry out gas-solid catalytic reaction in fluidized bed reactor 1, obtain mixed gas;

[0143] (b) the mixed gas that step (a) obtains obtains the methylaluminum chloride product after separation;

[0144] (c) The methylaluminum chloride product that step (b) obtains reacts with phosphorus trichloride in the synthesis unit 6 of methyl phosphorus dichloride to generate ligand 3CH 3 PCl 2 2AlCl 3 , and then react with an alkali metal halide to obtain methyl phosphorus dichloride;

[0145] (d) reacting the methyl phosphorus dichloride obtained in step (c) with alcohol to obtain a methyl phosphite product.

Embodiment 1

[0148] This embodiment provides a system for preparing methyl phosphite, such as figure 1 As shown, the system includes a methyl aluminum chloride synthesis unit, a methyl phosphorus dichloride synthesis unit and a methyl phosphite synthesis unit; the methyl aluminum chloride synthesis unit includes a fluidized bed reactor connected in sequence 1 and a separation unit, the methyl phosphorus dichloride synthesis unit includes a methyl phosphorus dichloride synthesis unit 6, and the methyl phosphorus dichloride synthesis unit 6 enters the separation for the product of the closed reactor fluidized bed reactor 1 The unit is separated, and the methylaluminum chloride obtained by the separation unit enters the methyl phosphorus dichloride synthesis unit 6 in the methyl phosphorus dichloride synthesis unit to react, and the methyl phosphorus dichloride synthesis unit obtains Phosphorous dichloride enters the synthesis unit of methyl phosphite;

[0149] Wherein, the bottom of the flu...

Embodiment 2

[0154] This embodiment provides a system for preparing methyl phosphite. The system structure refers to the system structure in Example 1, the difference is that the gas hole opening rate on the gas distributor 5 is 13.8%, and the fluidized bed reaction A U-shaped heat exchanger is set in the device 1, such as image 3 As shown, the U-shaped heat exchanger is placed above the gas distributor 6; the gas-solid separation device 2 is placed outside the fluidized bed reactor 1, and its solid material outlet is communicated from the outside of the fluidized bed reactor 1 to the Above the gas distributor in the fluidized bed reactor 1; the methyl phosphite synthesis unit 8 is a tubular reactor, and the deacidification unit 9 is a falling film evaporator.

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Abstract

The invention provides a system and a preparation method for preparing methyl phosphite by using methyl aluminum chloride, the system includes a methyl aluminum chloride synthesis unit, a methyl phosphorus dichloride synthesis unit and a methyl Phosphite synthesis unit; the methyl aluminum chloride synthesis unit includes a fluidized bed reactor and a separation unit connected in sequence, the methyl phosphorus dichloride synthesis unit includes a methyl phosphorus dichloride synthesis unit, and the methyl phosphorus dichloride The synthesis device is a closed reactor. The present invention carries out the gas-solid catalytic reaction in the fluidized bed reactor and optimizes the separation equipment to prepare the methyl aluminum chloride product, and then prepares the methyl phosphorus dichloride by using the methyl aluminum chloride as raw material, and then continuously synthesizes the methyl chloride Phosphate products. The yield of methyl phosphorus dichloride is improved, and then the yield of methyl phosphite product is improved, the operation is simple, basically no three wastes are generated, no solvent is needed, and it is green and environmentally friendly.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and relates to a system and method for preparing methyl phosphite, in particular to a method of preparing and separating methyl aluminum chloride in a fluidized bed reactor, and using the prepared methyl Aluminum chloride prepares methyl phosphorus dichloride in an improved reactor, and then prepares a system and a preparation method of methyl phosphite. Background technique [0002] Methyl phosphite is an important chemical raw material intermediate, which can be widely used in the preparation of flame retardants and herbicides. The methyl phosphite structure is shown below: [0003] CH 3 P(OR) n (OH) 2-n [0004] Wherein, the group R is an alkyl group with 1-4 C atoms, and n is 1 or 2. Such substances are widely used and can be used in the synthesis of flame retardants and pesticides. [0005] As a raw material for efficiently synthesizing methyl phosphite, methyl phosphine dich...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/48C07F5/06C07F9/52
CPCC07F9/4808C07F5/064C07F9/52
Inventor 周曙光秦龙李培国余神銮祝小红陈华涛徐亚卿
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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